Detergent product and process of making same



PRODUCT AND rnoonss G s Fnrness, Warrington, and Arthur Fairna'raaonn'r A FEE bourne, Bebington, England, era to Lever. Brothers Limited, Port Sunlight, England, a

company of Great Britain This invention relates to the manufacture of ,washing preparations and the like in the form of powders suitable for. domestic, textile and analogous uses.

6 As is mown, when glycerol is heated with or without acatahrst under suitable conditions, condensation occurs and so-called polyglycerols are produced. By partial esteriflcation of the polyglycerols with fatty acids the corresponding 10 esters-i.- e., esters containing unesterifled hydrowl groups-can be produced. Other methods of producing these esters are known; for example, by heating fats or oils (triglycerides) with glycerol in presence or absence of a catalyst undersuitable conditions, whereby condensation and esteriflcation are effected in one operation.

Esters of the aforementioned kind have been found to possess detergent properties, but their thick oily or syrupy consistency offers disadvantages from the practical point of view. Their behaviour towards water varies widely, some'being freely and others but slightly soluble in water. For the purpose of this invention the ester employed should be soluble in water to at least the extent required to produce a solution of adequate concentration for washing purposes (say a solution containing from about 0.02% to 0.2% as dissolved ester), although the presence of a small proportion of emulsified ester is not as a? rule objectionable. Esters corresponding approximately to mono-fatty acid esters of tri-. tetra-,and penta-glycerols have been found to give satisfactory results. The term "fatty acid" herein employed includes all soap-forming fatty acids and also rosin and naphthenic acids. The lower fatty acids, such as the mixed fatty acids of palm kernel oil, have yielded products of high Q detergent quality. The polyglycerol ester em-- ployed may eitherbe the crude unpurifled prodnot (as obtained directly by methods such as those mentioned above) containing a more or less considerable proportion of unconverted glycerol or polyglycerol, or it maybe a concentrated ester substantially free from such impurities.

The object of the invention is to produce from such esters'free-flowing detergent powders suitable for thedomestic and textile uses to which soap is commonly employed.

- According to this invention a process for the manufacture of a washing preparationinv the form of a powder suitable for domestic, textile and analogous usesconsists in intimately incorporating a soluble polyglycerol ester containing unesterified hydroxyl groups with a suitable solu- 8 Claims. (oi. iii-5).

ble sulphate or mixture of such sulphates, with or without the addition of soluble alkali metaphosphate and/or alkali pyrophosphate.

The powders thus obtained possess strong .detergent properties, lather freely, are limeresistant and are well adapted for use in domestic,

laundry or industrial washing, cleansing and the like.

Suitable soluble sulphates are the sulphates of sodium, potassium, ammonium and magnesium.

Since, however, magnesium sulphate reacts with alkali pyrophosphate, forming an insoluble precipitate, these two salts should not be used in conjunction unless soluble alkali metaphosphate is also present.in quantity suflicient to prevent formation of this precipitate.

The efliciency of the various salts and salt mix-' tures is not the same in respect of all polyglycerol esters. Their suitability for use and the proportions in which they should be used depend upon purity of the latter.

scale in the light of the examples hereinafter given will show which of the particular salts or salt mixtures and what proportion thereof are best suited for converting the particular ester into the desired free-flowing powder. As a. general rule dryness and freedom of flow improve with increasing proportion of'salts. Satisfactory products of high detergent power and pleasant appearance. havp been obtained by using .one part of polyglycerol ester and, for example, 2 to 4 .parts by weight of the above-mentioned salts,

particularly satisfactory powders having been obtained by incorporating one part of concentrated, purified ester with 4v parts of sodium sulphate (NMSOO Magnesium sulphate when used is preferably in the form of its crystalline salt MgSO4.7I-I2O.

. which, however, loses the major part of its water of crystallisation during the drying stage of the tion of water and then quickly drying the intimate mixture in such manner that the esterdoes not have an opportunity of separating from it before. drying is completed. This is best effected by spray drying the mixture'or drying it steam-heated rotaryv cylinder.

Example I The following example illustrates the production, according to the invention, of a detergent powder from a crude ester containing unconverted glycerol and polyglycerol which was obtained by partly esterifying polyglycerol (approximately penta-glycerol) with per cent.

of the mixed fatty acids from coconut oil. A

mixture of sodium sulphate (l /r3 parts), soluble sodium metaphosphate part), sodium pyrophosphate (V A part) and water (from 2 to 4 parts) was heated with stirring to near 80 C. When all the metaphosphate and part or all of the other salts had dissolved, the mixture was cooled to about 50 C., the crude ester (1 part) was added, the whole was agitated and cooled to below 35 C., whereupon the well-agitated thick cream formed was fed on to the surface of a rotary drying cylinder heated internally with steam at about 20 lb. pressure. The dried product removed from the cylinder formed a powder of very satisfactory quality, containing about 3% of water and having the composition:

v Parts Crude ester 1 Sodium metaphosphate; /2 Sodium pyrophosphate A; /2 Sodium sulphate (Na2SO4) 1 /23 Example II The following example illustrates the production, according to the invention, of a detergent powder from-a. purified ester which was prepared by removing substantially the whole of the unconverted glycerol and polyglycerol from a crude ester obtained as mentioned in the foregoing example. Soluble sodium metaphosphate (Mi-V2 part) was dissolved in water (1 %-2 parts) and to the solution were added sodium sulphate (2 parts) and purified ester (1 part) along with a further quantity of water sufiicient to give a cream of suitable consistency when the mixture was cooled. The vigorously stirred cream was then dried on a rotary drying cylinder as in the foregoing example. The somewhat sticky product was mixed intimately with suflicient sodium sulphate and sodium pyrophosphate to yield a final product in the form of a dry, freeflowing powder having 'the composition:

Parts Polyglycerol ester 1 Sodium metaphosphate /8-- /2 Sodium pyrophosphate /2 Sodium sulphate (NazSOo 3-5 Example III The following example illustrates the production, according to the invention, of a detergent powderby the spray-drying method. The polyglycerol ester is mixed with the salt and a suflicient quantity of water in a crutcher, and the mass then cooled until a smooth stable cream is formed. The quantity of water varies to some extent with the solubility of the salt but is in general between to 40% of the crutcher charge. The cream is then sprayed into hot air at 260 C. to 270 C. whereby dry powders, consisting in many cases of light and puffed particles, are obtained.

We claim:

1. A detergent product which is in the form of a dry free-flowing powder and comprises a substantially water-soluble polyglycerol fatty acid ester containing unesterified hydroxyl groups, said ester being normally of viscous consistency, in intimate admixture with at least one of the soluble sulphates selected from thegroup consisting of sodium sulphate, potassium sulphate, ammonium sulphate and magnesium sulphate, the quantity of soluble sulphate being suflicient to constitute the product dry and free-flowing.

2. A detergent product which is in the form of a dry free-flowing powder and comprises a substantially water-soluble polyglycerol fatty acid ester containing unesterified hydroxyl groups, said ester being normally of viscous con-' sistency. in intimate admixture with at least 'one of the soluble sulphates selected from the group consisting of sodium sulphate, potassium sulphate, ammonium sulphate and magnesium sulphate, together with a water soluble alkali metal metaphosphate, the quantity of solublesulphate being suflicient to constitute the product dry and free-flowing. I

3. A detergent product which is in the form of a dry free-flowing powderand comprises a substantially water-soluble polyglycerol fatty acid ester containing unesterified hydroxyl groups,

said ester being normally of viscous consistency,

in intimate admixture with at least one of the soluble sulphates selected from the group con-v sisting of sodium sulphate, potassium sulphate, ammonium sulphate and magnesium sulphate, together with a water soluble alkali metal metaphosphate, and an alkali metal pyrophosphate, the quantity of soluble sulphate being suflicient to constitute the product dry and free-flowing, and the quantity of metaphosphate being sufficient to prevent the formation of an insoluble precipitate of magnesium pyrophosphate.

4. A detergent product which is in the form of a dry free-flowing powder and comprises a substantially water-soluble polyglycerol fatty acid ester containing unesterified hydroxyl groups, said ester being normally of viscous consistency. in intimate admixture with at least one of the soluble sulphates selected from the group consisting of sodium sulphate, potassium sulphate, and ammonium sulphate, together with an alkali metal pyrophospham, the quantity of soluble sulphate being suflicient to constitute the product dry and free-flowing.

5. A detergent product which is in the form of a dry free-flowing ,powder and comprises 1 part by weight of a substantially water-soluble polyglycerol fatty acid ester containing unesterifled hydroxyl groups, said ester being normally of viscous consistency, and 2 to 4 parts by weight of a soluble sulphate selected from the group consisting of sodium sulphate, potassium sulphate, ammonium sulphate and magnesium sulphate.

' 6. A process for the production of a dry freeflowing detergent powder comprising intimately incorporating 1 part by weight of a substantially water-soluble polyglycerol fatty acid ester containing unesterifled hydroxyl groups, said ester being normally of viscous consistency, with 2 parts by weight of sodium sulphate, and $4; to V part by weight of sodium metaphosphate, by mixing the ingredients with 1% to 2 parts by weight of water to form a stable magma, quickly drying the mixture with the influence of heat.

substantially water-soluble polyglycerol fatty acid' ester containing unesterified hydroxyi groups,

' said ester being normally of viscous consistency,

with at least one of the soluble sulphates selected from the group consisting of sodium sulphate, potassium sulphate, ammonium sulphate, and magnesium sulphate, and water in such quantity as will produce a stable mama, and quickly drying the mixture with the influence of heat. the quantity of soluble sulphate being sufllcient to obtain the final product as a dry free-flowing powder.

8. A process for the production of a dry freeflowing detergent powder comprising mixing a substantially water-soluble polyglycerol fatty acid ester containing unesterifled hydroxyl groups, said ester being normally of viscous consistency, with at least one of the soluble sulphates selected from the group consisting of sodium sulphate, potassium sulphate, ammonium sulphate, and magnesium sulphate, and water in such quantity as will produce a stable magma, and spray drying the mixture, the quantity of soluble sulphate being suflicient to obtain the final product as a dry free-flowing powder.

REGINALD FURNESS. ARTHUR FAIRBOURNE. 

